CN109180866A - A kind of preparation method for the Petropols that melt viscosity is controllable - Google Patents
A kind of preparation method for the Petropols that melt viscosity is controllable Download PDFInfo
- Publication number
- CN109180866A CN109180866A CN201810940907.4A CN201810940907A CN109180866A CN 109180866 A CN109180866 A CN 109180866A CN 201810940907 A CN201810940907 A CN 201810940907A CN 109180866 A CN109180866 A CN 109180866A
- Authority
- CN
- China
- Prior art keywords
- component
- fraction
- isolated
- preparation
- isoprene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F240/00—Copolymers of hydrocarbons and mineral oils, e.g. petroleum resins
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of preparation methods of Petropols that melt viscosity is controllable.This method comprises the following steps: (1) the isolated pentadiene component of C5 fraction, thick isoprene component, monoene the hydrocarbon component and polymerization grade isoprene component being added in solvent and mixed, mixed feed components are obtained, catalyst is added and carries out polymerization reaction；(2) after reaction, cool down, demulsifier Removal of catalyst, washing is added, then remove solvent, stripping removing oligomer obtains the controllable Petropols of the melt viscosity.The Petropols of the method for the present invention preparation can produce the Petropols of different melt viscosities under the premise of meeting product softening point stabilization to meet the needs of different application field；Meanwhile preparation method of the invention is simple to operation, mild condition is conducive to large-scale industrial production.
Description
Technical field
The present invention relates to Petropols preparation technical fields, and in particular to a kind of system for the Petropols that melt viscosity is controllable
Preparation Method.
Background technique
Petropols are the good resins of low molecular weight, thermoplasticity, and molecular weight is generally in 300-3000, since it has price low
It is honest and clean, that acid value is small, compatibility is good, fusing point is low, water-fast, resistance to ethyl alcohol and chemicals and having adjusts viscosity and thermal stability is good etc. is excellent
Point is widely used in including a variety of industries such as rubber, adhesive, coating, papermaking and ink and field.
Isolated pentadiene, isoprene and bicyclic penta 2 can be passed through from the light dydrocarbon raw material of cracking of ethylene by-product
The fractions such as alkene can further obtain C 5 petroleum resin by polymerization.The Petropols manufactured using the prior art, softening point are general
All at 90~100 DEG C, melt viscosity is at 160 DEG C of 500~1000cps@.
Softening point is the major influence factors of Petropols melt viscosity, and other influence factors include molecular weight and molecular weight
Distribution, molecular structure etc..Petropols are all anxious related to its softening point in the application of many fields and industry.Meeting
Under the premise of Petropols softening point, on the one hand in some application fields, such as high melt viscosity modified pitch, it is desirable to product tool
There is biggish melt viscosity；On the other hand in the adhesive tapes such as label field, it would be desirable that the lesser melt viscosity of product is produced with improving
Product just glue and production efficiency.In addition, there are also some fields, it would be desirable that resin has more moderate melt viscosity so that product reaches
The balance of production efficiency and service performance.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of Petropols that melt viscosity is controllable
Preparation method.This method is to realize melt viscosity under the premise of stablizing softening point by adjusting formula and processing technology
The preparation of controllable Petropols produces the petroleum tree of different melt viscosities under the premise of meeting product softening point stabilization
Rouge is to meet the needs of different application field.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method for the Petropols that melt viscosity is controllable, includes the following steps:
(1) by the isolated pentadiene component of C5 fraction, thick isoprene component, monoene the hydrocarbon component and polymerization
Grade isoprene component, which is added in solvent, to be mixed, and mixed feed components are obtained, and is added catalyst and is carried out polymerization reaction；
(2) after reaction, cool down, demulsifier Removal of catalyst, washing is added, then remove solvent, stripping removing is oligomeric
Object obtains the controllable Petropols of the melt viscosity.
Preferably, in step (1), in the isolated pentadiene component of the C5 fraction, the concentration of pentadiene
For 55~80wt%.
It is furthermore preferred that in step (1), in the isolated pentadiene component of the C5 fraction, pentadiene it is dense
Degree is 65~75wt%.
Preferably, in step (1), in the isolated thick isoprene component of the C5 fraction, isoprene it is dense
Degree is 30~70wt%.
It is furthermore preferred that in step (1), in the isolated thick isoprene component of the C5 fraction, isoprene
Concentration is 40~70wt%.
Preferably, in step (1), in the isolated monoene the hydrocarbon component of the C5 fraction, the concentration of monoolefine is 30
~70wt%.
It is furthermore preferred that in the isolated monoene the hydrocarbon component of the C5 fraction, the concentration of monoolefine is in step (1)
45~60wt%.
Preferably, in step (1), in the isolated polymerization grade isoprene component of the C5 fraction, isoprene
Concentration be greater than 99.5wt%.
By the additional amount for controlling each component, it is ensured that the amount of isoprene is controlled 0~40%, preferably in raw mixture
It is 10~30%.
Preferably, in step (1), the solvent includes one or more of saturated alkane and saturation aromatic hydrocarbon.
It is furthermore preferred that the saturated alkane includes pentane, n-hexane, hexamethylene or normal heptane.
It is furthermore preferred that the saturation aromatic hydrocarbon includes toluene, ethylbenzene, dimethylbenzene or trimethylbenzene.
Preferably, in step (1), by mass percentage, the additional amount of each component are as follows: penta between C5 fraction is isolated
10~50wt% of diene component, the isolated 0~50wt% of thick isoprene component of C5 fraction, C5 fraction are isolated
Monoene 10~70wt% of the hydrocarbon component, the isolated polymerization grade isoprene 0~20wt% of component of C5 fraction, solvent 10~
50wt%, the percentage summation of each component are 100wt%.
Preferably, in step (1), the catalyst includes AlCl3Or BF3。
It is furthermore preferred that the catalyst is AlCl in step (1)3, partial size is 20~100 mesh.
Preferably, in step (1), the additive amount of the catalyst is 0.5~2.0wt% of mixed feed components, more excellent
It is selected as 0.9~1.5wt%.
Preferably, in step (1), the temperature of the polymerization reaction is 20~110 DEG C, and the time is 90~300min.
It is furthermore preferred that the temperature of the polymerization reaction is 40~80 DEG C in step (1), the time is 120~240min.
Preferably, in step (2), the demulsifier include isopropanol, BASF AG the trade mark be DB9393, L31,
One or more of the demulsifier of L61 and P105.
Preferably, in step (2), the dosage of the demulsifier is 50~1000ppm of mixture after reaction.
Preferably, in step (2), the washing is that washing to cleaning solution is in neutrality；The stripping is using 200~300
DEG C vapor is stripped.
Compared with prior art, the invention has the advantages that and the utility model has the advantages that
The Petropols of the method for the present invention preparation can produce different meltings under the premise of meeting product softening point stabilization
The Petropols of viscosity are to meet the needs of different application field；Meanwhile preparation method of the invention is simple to operation, condition temperature
Be conducive to large-scale industrial production.
Specific embodiment
Technical solution of the present invention is described in further detail below in conjunction with specific embodiment, but protection of the invention
Range and embodiment are without being limited thereto.
In specific embodiment, the method for preparing the controllable Petropols of melt viscosity specifically comprises the following steps:
(1) by the isolated pentadiene component of C5 fraction, thick isoprene component, monoene the hydrocarbon component and polymerization
Grade isoprene component is added in material-compound tank, is uniformly mixed, spare；
(2) hexamethylene is added in 2L reaction kettle, each component that the additional amount of hexamethylene is isolated with C5 fraction adds
The percentage summation for entering amount is 100wt%；Add the catalyst AlCl that partial size is 20 mesh3, starting is stirred and is heated up, after heating
It starts charge pump and the material that step (1) is mixed to get is transferred to reaction kettle progress polymerization reaction 180min；
(2) after reaction, 45 DEG C are cooled to, BASF AG's trade mark of mixture 100ppm after reaction is added
For the demulsifier of DB9393, Removal of catalyst, washing removes non-polycondensation monomer at 150 DEG C, then removes solvent, is passed through 260 DEG C of saturations
Vapor stripping removing oligomer, obtains the controllable Petropols of the melt viscosity.
Wherein, the isolated pentadiene component (component A) of the C5 fraction of use, thick isoprene component (component
B), the composition of monoene the hydrocarbon component (component C) and polymerization grade isoprene component (component D) is respectively as shown in 1~table of table 4.
The isolated pentadiene component (component A) of 1 C5 fraction of table
The isolated thick isoprene component (component B) of 2 C5 fraction of table
The isolated monoene the hydrocarbon component (component C) of 3 C5 fraction of table
The isolated polymerization grade isoprene component (component D) of 4 C5 fraction of table
In specific embodiment, to the softening points of the Petropols being prepared, fusion viscosimeter coloration according to following
Testing standard or test method carry out respective performances test:
(1) softening point: GB/T 4507-1999；
(2) melt viscosity: HG/T 3660-1999；
(3) coloration: the Petropols and toluene of preparation are prepared according to quality 1:1, after dissolution completely, are used
The UltraScan Pro D65 type colour photometer of HunterLab company carries out the test of mixed liquor, and is indicated with yellow colour index.
In specific embodiment, also compared using commercially available universal sample.Wherein, E-1304 and E-1310 is Ai Ke
The softening point of two kinds of trade mark Petropols of gloomy Mobil Corporation, E-1304 and E-1310 are respectively 99.2 DEG C and 93.0 DEG C.
Examples 1 to 10
Wherein, polymerization temperature is 60 DEG C, and catalyst amount is 1.2wt%, remaining condition and specific embodiment are retouched
It states identical.The performance indicator of the Petropols of the additive amount and preparation of component A~D of Examples 1 to 10 is as shown in table 5.
The performance indicator of the Petropols of the additive amount and preparation of component A~D of 5 Examples 1 to 10 of table
As shown in Table 5, the trade mark of the Exxon Mobil Corporation more common with existing market is the Petropols of E-1304
Compare, Examples 1 to 10 preparation Petropols guarantee softening point close in the case where, with isoprene additive amount increasing
Add, biggish raising occurs in the melt viscosity of the Petropols of preparation.
Embodiment 11~17
Wherein, polymerization temperature is 60 DEG C, and catalyst amount is 1.2wt%, remaining condition and specific embodiment are retouched
It states identical.The performance indicator of the Petropols of the additive amount and preparation of component A~D of embodiment 11~17 is as shown in table 6.
The performance indicator of the Petropols of the additive amount and preparation of component A~D of 6 embodiment 11~17 of table
As shown in Table 6, the trade mark of the Exxon Mobil Corporation more common with existing market is the Petropols of E-1310
Compare, Petropols prepared by embodiment 11~17 guarantee softening point close in the case where, with the increase of isoprene pair,
There is biggish raising in the melt viscosity of the Petropols of preparation.
Embodiment 18~22
It is same as Example 7, tested under different polymerization temperatures, the polymeric reaction temperature of embodiment 18~22 and
The performance indicator of the Petropols of preparation is as shown in table 7.
The performance indicator of the Petropols of the polymeric reaction temperature and preparation of 7 embodiment 18~22 of table
As shown in Table 7, compared with Petropols prepared by embodiment 7, Petropols prepared by embodiment 18~22 are being protected
In the case that card product softening point is stablized, with the raising of reaction temperature, under the viscosity of the Petropols of preparation occurs significantly
Drop.
Above embodiments are only preferred embodiment of the invention, are only that further detailed to technical solution of the present invention work
Description, but protection scope of the present invention and embodiment are without being limited thereto, any without departing under spirit of the invention and principle
Change, combination, deletion, replacement or modification for being made etc. are included in protection scope of the present invention.
Claims (10)
1. a kind of preparation method for the Petropols that melt viscosity is controllable, which comprises the steps of:
(1) the isolated pentadiene component of C5 fraction, thick isoprene component, monoene the hydrocarbon component and polymer grade is different
Pentadiene component, which is added in solvent, to be mixed, and mixed feed components are obtained, and is added catalyst and is carried out polymerization reaction；
(2) after reaction, cool down, demulsifier Removal of catalyst, washing is added, then remove solvent, stripping removing oligomer obtains
The Petropols controllable to the melt viscosity.
2. preparation method according to claim 1, which is characterized in that in step (1), the C5 fraction is isolated
In pentadiene component, the concentration of pentadiene is 55~80wt%；The isolated thick isoprene component of the C5 fraction
In, the concentration of isoprene is 30~70wt%；In the isolated monoene the hydrocarbon component of the C5 fraction, the concentration of monoolefine
For 30~70wt%；In the isolated polymerization grade isoprene component of the C5 fraction, the concentration of isoprene is greater than
99.5wt%。
3. preparation method according to claim 1, which is characterized in that in step (1), the C5 fraction is isolated
In pentadiene component, the concentration of pentadiene is 65~75wt%；The isolated thick isoprene component of the C5 fraction
In, the concentration of isoprene is 40~70wt%；In the isolated monoene the hydrocarbon component of the C5 fraction, the concentration of monoolefine
For 45~60wt%；In the isolated polymerization grade isoprene component of the C5 fraction, the concentration of isoprene is greater than
99.5wt%。
4. preparation method according to claim 1, which is characterized in that in step (1), the solvent include saturated alkane with
And one or more of saturation aromatic hydrocarbon.
5. preparation method according to claim 1, which is characterized in that in step (1), by mass percentage, each component
Additional amount are as follows: the isolated pentadiene 10 ~ 50wt% of component of C5 fraction, the isolated thick isoprene of C5 fraction
0 ~ 50wt% of component, the isolated monoene 10 ~ 70wt% of the hydrocarbon component of C5 fraction, the isolated polymer grade isoamyl of C5 fraction
0 ~ 20wt% of diene component, 10~50wt% of solvent.
6. preparation method according to claim 1, which is characterized in that in step (1), the catalyst includes AlCl3Or
BF3；The additive amount of the catalyst is 0.5~2.0wt% of mixed feed components.
7. preparation method according to claim 1, which is characterized in that in step (1), the temperature of the polymerization reaction is 20
~110 DEG C, the time is 90~300min.
8. preparation method according to claim 1, which is characterized in that in step (1), the temperature of the polymerization reaction is 40
~80 DEG C, the time is 120~240min.
9. preparation method according to claim 1, which is characterized in that in step (2), the demulsifier include isopropanol,
The trade mark of BASF AG is one or more of the demulsifier of DB9393, L31, L61 and P105；The dosage of the demulsifier is
50~1000ppm of mixture after reaction.
10. preparation method according to claim 1, which is characterized in that in step (2), the cooling is to be cooled to 40 ~ 50
℃；The washing is that washing to cleaning solution is in neutrality；The stripping is stripped using 200 ~ 300 DEG C of vapor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810940907.4A CN109180866A (en) | 2018-08-17 | 2018-08-17 | A kind of preparation method for the Petropols that melt viscosity is controllable |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810940907.4A CN109180866A (en) | 2018-08-17 | 2018-08-17 | A kind of preparation method for the Petropols that melt viscosity is controllable |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109180866A true CN109180866A (en) | 2019-01-11 |
Family
ID=64918232
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810940907.4A Pending CN109180866A (en) | 2018-08-17 | 2018-08-17 | A kind of preparation method for the Petropols that melt viscosity is controllable |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109180866A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3893986A (en) * | 1972-10-12 | 1975-07-08 | Nippon Zeon Co | Process for the preparation of novel hydrocarbon resins |
| CN108219068A (en) * | 2018-01-10 | 2018-06-29 | 安徽同心化工有限公司 | Controllable high-performance polymer resin of a kind of melt viscosity and preparation method thereof |
-
2018
- 2018-08-17 CN CN201810940907.4A patent/CN109180866A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3893986A (en) * | 1972-10-12 | 1975-07-08 | Nippon Zeon Co | Process for the preparation of novel hydrocarbon resins |
| CN108219068A (en) * | 2018-01-10 | 2018-06-29 | 安徽同心化工有限公司 | Controllable high-performance polymer resin of a kind of melt viscosity and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 宁媛媛: "间戊二烯石油树脂聚合工艺研究", 《石油化工应用》 * |
| 王世雄: "浅析间戊二烯石油树脂的合成", 《黑龙江科技信息》 * |
| 高富业等: "C5石油树脂生产工艺的改进", 《石油化工》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4677176A (en) | Light color, low softening point petroleum hydrocarbon resins | |
| CN108774296A (en) | A kind of preparation method of modified petroleum resin | |
| CN109180866A (en) | A kind of preparation method for the Petropols that melt viscosity is controllable | |
| CN109232894A (en) | Methoxy group methyl phenyl silicone resin, organosilicon coating glue and preparation method and application | |
| CN1064376C (en) | Process for manufacturing isoprene containing block copolymers | |
| CN109721828A (en) | A kind of high heat resistance and cold-resistant high-gloss metal texture are exempted to spray PP material and preparation method thereof | |
| CN104892840B (en) | A kind of phenylethene modified dicyclopentadiene petroleum resin and preparation method thereof | |
| KR20190096520A (en) | Method for preparing conjugated diene based polymer and apparatus for preparing conjugated diene based polymer | |
| US4684707A (en) | Low color, high softening point aromatic resin and method for its production | |
| JP5720109B2 (en) | Method for producing episulfide compound | |
| CN104276915A (en) | Separation method for C9-C10 fractions | |
| CN103509575A (en) | Solvent used for preparation of high-quality coal-based needle coke | |
| US2994689A (en) | Utilization of high boiling fractions in preparing petroleum resins | |
| CN103725318B (en) | A kind of production method of aromatic hydrocarbon rubber extender oil | |
| CN102676214A (en) | Solvent refining method and equipment for producing environmental-protection rubber filling oil | |
| US2230274A (en) | Purification of valuable hydrocarbons | |
| CN109694729B (en) | Preparation method of white oil | |
| CN107286286A (en) | A kind of acrylic resin and its preparation technology for mending paint coating | |
| EP0063419A1 (en) | Process for preparing light colored petroleum resins and resins produced thereby | |
| JPH01144407A (en) | Hydrogenated liquid aliphatic hydrocarbon resin | |
| CN110923005A (en) | Preparation method of high-boiling-point aromatic hydrocarbon solvent | |
| CN109306036A (en) | A kind of cold poly- production method of Petropols reducing gel | |
| CN106083663B (en) | A kind of method for improving stannous methanesulfonate product clarity | |
| JPH02124913A (en) | Preparation of coumarone resin | |
| CN105219106B (en) | One kind cleaning RX |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: 516081 No. 328, Aotou Petrochemical Avenue, Daya Bay, Huizhou City, Guangdong Province Applicant after: Huizhou iske new material technology development Co.,Ltd. Address before: 516081 No. 328, Aotou Petrochemical Avenue, Daya Bay, Huizhou City, Guangdong Province Applicant before: HUIZHOU DAYA BAY YIKESI NEW MATERIAL TECHNICAL Co.,Ltd. |
|
| CB02 | Change of applicant information | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190111 |
|
| RJ01 | Rejection of invention patent application after publication |